Oxygen → Isobutene Isobornyl Acrylate

HRID 1264143

반응식

HRID 1264143 반응식
[CH3:1][C@@:2]12[CH:10]([C:11]([C:13]([O-:15])=[O:14])=[CH2:12])[CH2:9][C@H:5]([C:6]1([CH3:8])[CH3:7])[CH2:4][CH2:3]2.CCCCC(C1C=CN=C(C2C=C(C(CCCC)CCCC)C=CN=2)C=1)CCCC.O=O>>[CH2:1]=[C:2]([CH3:6])[CH3:3].[CH3:1][C@@:2]12[CH:10]([C:11]([C:13]([O-:15])=[O:14])=[CH2:12])[CH2:9][C@H:5]([C:6]1([CH3:7])[CH3:8])[CH2:4][CH2:3]2

참가 물질

4

반응물 3

HCID 977OxygenHCID 1749844,4'-Bis(1-butylpentyl)-2,2'-bipyridineHCID 92004758Isobomyl acrylate3회

생성물 1

HCID 131723834Isobutene Isobornyl Acrylate

반응 조건

온도
0 °C

실험 절차

The following reagents were weighed into a glass tube under ambient temperature: 0.3 g(3×10−7 mol) brominated p-methylstyrene-isobutene elastomer (Exxon) (Mn=108380, Mw/Mn=2.31), 12 mg (8.37×10−2 mmol) of CuBr, 1.00 mL (0.986 g, 5 mmol) of isobornyl acrylate, and 60 mg (0.175 mmol) 4,4′-di-(5-nonyl)-2,2′-bipyridine. Two “freeze-pump-thaw” cycles were performed on the contents of the tube to insure that oxygen was removed from the polymerization solution. The tube was sealed under vacuum and placed in an oil bath thermostated at 90 C. After 2 h the tube was removed from the oil bath and cooled to 0° C. to quench the polymerization. Conversion of the monomer was measured using GC; the molecular weight and polydispersity were measured by GPC. Conversion of isobornyl acrylate was 30%, Mn=141000, Mw/Mn=2.61. 1H NMR spectrum showed that the graft copolymer contained 30% isobornyl acrylate. By DSC measurement one Tg was found at 2° C.

후처리

  1. customThe following reagents were weighed into a glass tube under ambient temperature
  2. customwas removed from the polymerization solution
  3. customThe tube was sealed under vacuum
  4. customplaced in an oil bath
  5. customAfter 2 h the tube was removed from the oil bath
  6. customto quench
  7. customthe polymerization
  8. customwas found at 2° C.

출처 및 근거

ORD 기록
ord-98f2a43f81434cc98a32c293427376a6
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06541580B1

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